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CN105542019B - Resistant dextrin and preparation method thereof - Google Patents
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CN105542019B - Resistant dextrin and preparation method thereof - Google Patents

Resistant dextrin and preparation method thereof Download PDF

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CN105542019B
CN105542019B CN201610055348.XA CN201610055348A CN105542019B CN 105542019 B CN105542019 B CN 105542019B CN 201610055348 A CN201610055348 A CN 201610055348A CN 105542019 B CN105542019 B CN 105542019B
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dextrin
resistant dextrin
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CN105542019A (en
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李方华
邵先豹
窦光鹏
干昭波
杨腾腾
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Shandong Bailong Park Biological Polytron Technologies Inc
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Priority to PCT/CN2017/071337 priority patent/WO2017128984A1/en
Priority to US15/566,234 priority patent/US10479840B2/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B30/00Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
    • C08B30/12Degraded, destructured or non-chemically modified starch, e.g. mechanically, enzymatically or by irradiation; Bleaching of starch
    • C08B30/18Dextrin, e.g. yellow canari, white dextrin, amylodextrin or maltodextrin; Methods of depolymerisation, e.g. by irradiation or mechanically
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/30Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/20Reducing nutritive value; Dietetic products with reduced nutritive value
    • A23L33/21Addition of substantially indigestible substances, e.g. dietary fibres
    • A23L33/25Synthetic polymers, e.g. vinylic or acrylic polymers
    • A23L33/26Polyol polyesters, e.g. sucrose polyesters; Synthetic sugar polymers, e.g. polydextrose
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/10Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/18Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns
    • B01D15/1864Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns using two or more columns
    • B01D15/1871Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns using two or more columns placed in series
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/26Selective adsorption, e.g. chromatography characterised by the separation mechanism
    • B01D15/36Selective adsorption, e.g. chromatography characterised by the separation mechanism involving ionic interaction, e.g. ion-exchange, ion-pair, ion-suppression or ion-exclusion
    • B01D15/361Ion-exchange
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B31/00Preparation of derivatives of starch
    • C08B31/003Crosslinking of starch
    • C08B31/006Crosslinking of derivatives of starch
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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Abstract

The present invention relates to a kind of resistant dextrin and preparation method thereof.The resistant dextrin, molar content≤7.0% of molar content≤4.5%, DP3 of DP1 molar content≤1%, DP2, average degree of polymerization is 6~12, pH value 3.0~6.0, dietary fiber molar content >=85%.The invention further relates to the preparation method of above-mentioned resistant dextrin.Dextrinization reaction is divided into two stages by the present invention first using starch as raw material, it is effectively guaranteed that the degree of polymerization of polymerisation, while reducing the generation of side reaction, greatly reduces the difficulty of purifying subsequent treatment.

Description

抗性糊精及其制备方法Resistant dextrin and its preparation method

技术领域technical field

本发明涉及一种抗性糊精及其制备方法,属于食品添加剂生产技术领域。The invention relates to a resistant dextrin and a preparation method thereof, belonging to the technical field of food additive production.

背景技术Background technique

随着人们生活水平的提高,很多人出现了高血脂、高血压、高血糖症状,俗称“三高”,且有越来越年轻化得趋势。世界卫生组织曾明确提出,防治心血管病的第一道防线就是减少“三高”和控制“三高”。这些三高的人群中,除了情况较严重的需要配合药物治疗外,大部分人群可以通过饮食食疗等方式进行调理,避免药物的副作用。With the improvement of people's living standards, many people have symptoms of hyperlipidemia, high blood pressure, and hyperglycemia, commonly known as the "three highs", and they tend to become younger and younger. The World Health Organization has clearly stated that the first line of defense in the prevention and treatment of cardiovascular disease is to reduce and control the "three highs". Among these people with three highs, except for those who are more serious and need to cooperate with drug treatment, most of them can be adjusted through diet therapy and other methods to avoid the side effects of drugs.

膳食纤维是一种不能被人体消化的碳水化合物,分为非水溶性和水溶性纤维两大类。国家在“十二五”规划当中,倡导发展膳食纤维的应用,遏制慢性病对国人造成的潜在危害,国际相关组织推荐的膳食纤维素日摄入量为:美国防癌协会推荐标准为每人每天30~40克,欧洲共同体食品科学委员会推荐标准为每人每天30克。中国营养学会推荐:人体每日膳食纤维摄入量为25-35克。Dietary fiber is a carbohydrate that cannot be digested by the human body. It is divided into two categories: insoluble and water-soluble fiber. In the "Twelfth Five-Year Plan", the country advocates the development of dietary fiber applications to curb the potential harm caused by chronic diseases to Chinese people. The daily intake of dietary fiber recommended by relevant international organizations is: the recommended standard of the American Cancer Prevention Association is per person per day 30-40 grams, the recommended standard of the European Community Food Science Committee is 30 grams per person per day. The Chinese Nutrition Society recommends that the daily dietary fiber intake for the human body is 25-35 grams.

抗性糊精是一种低热量葡聚糖,以天然淀粉为原料制备的低分子水溶性膳食纤维,相对于其他膳食纤维产品,抗性糊精具有良好的酸、热稳定性,高消化耐受性,低血糖指数,低胰岛素指数,热量低,防止龋齿等优异的特性。Resistant dextrin is a low-calorie dextran, a low-molecular water-soluble dietary fiber prepared from natural starch. Compared with other dietary fiber products, resistant dextrin has good acid and heat stability and high digestion resistance. Acceptability, low glycemic index, low insulin index, low calorie, prevent dental caries and other excellent properties.

中国专利文献CN 104403009 A(申请号201410671093.0)公开了一种抗性糊精的制备方法,包括以下步骤:以经酸处理后的淀粉为原料,采用海砂为传热介质,在高温条件下进行热解反应,获得焦糊精粗品,焦糊精粗品再经过精制处理得到抗性糊精产品。Chinese patent document CN 104403009 A (application number 201410671093.0) discloses a method for preparing resistant dextrin, which includes the following steps: using acid-treated starch as a raw material, using sea sand as a heat transfer medium, and carrying out the process under high temperature conditions. Pyrolysis reaction to obtain crude pyrodextrin, which is then refined to obtain resistant dextrin products.

中国专利文献CN103725732A(申请号201310743226.6)公开了一种小麦C淀粉综合利用制备抗性糊精的方法,包括以下步骤:(1)以小麦淀粉C淀粉浆为原料,用盐酸调pH后,密封酸化;(2)将酸化过的淀粉浆离心后干燥;(3)在滚子加热炉中高温裂解;(4)冷却至室温,加入适量的蒸馏水,调制成一定浓度范围的乳状液;(5)双酶协同法液化糖化同步进行;(6)加活性炭脱色并抽滤得到样液;(7)将料液进行醇沉,离心,上清液蒸馏酒精回收循环利用,沉淀进行气流干燥,得到含量为85%-90%的抗性糊精,产品收率为80%-90%。Chinese patent document CN103725732A (application number 201310743226.6) discloses a method for comprehensive utilization of wheat starch C to prepare resistant dextrin, comprising the following steps: (1) using wheat starch C starch slurry as raw material, adjusting the pH with hydrochloric acid, sealing and acidifying (2) drying the acidified starch slurry after centrifugation; (3) pyrolysis in a roller heating furnace; (4) cooling to room temperature, adding an appropriate amount of distilled water, and preparing an emulsion with a certain concentration range; (5) The double-enzyme synergistic method of liquefaction and saccharification is carried out simultaneously; (6) add activated carbon for decolorization and suction filtration to obtain the sample liquid; (7) carry out alcohol precipitation on the feed liquid, centrifuge, and recycle the supernatant by distilling alcohol, and air-dry the precipitation to obtain the content The resistance dextrin is 85%-90%, and the product yield is 80%-90%.

上述制备方法仍存在产品苦味大、易潮解、流动性差等缺点,无法在食品、保健品广泛的应用,尤其是高端食品和保健品领域。The above-mentioned preparation method still has the disadvantages of high bitterness, deliquescence, and poor fluidity of the product, and cannot be widely used in food and health products, especially in the fields of high-end food and health products.

发明内容Contents of the invention

本发明针对现有技术的不足,提供一种抗性糊精及其制备方法。经本发明制备的抗性糊精不易潮解,具有良好的口感和流动性,便于在食品、保健品尤其是高端食品和保健品领域广泛应用。Aiming at the deficiencies of the prior art, the invention provides a resistant dextrin and a preparation method thereof. The resistant dextrin prepared by the invention is not easy to deliquescence, has good taste and fluidity, and is convenient for wide application in the fields of food and health care products, especially high-end food and health care products.

术语说明Glossary

DP是指聚合度(Degree of Polymerization),是衡量聚合物分子大小的指标,以重复单元数为基准,即聚合物大分子链上所含重复单元数目的平均值。DP refers to the degree of polymerization (Degree of Polymerization), which is an index to measure the molecular size of a polymer, based on the number of repeating units, that is, the average number of repeating units contained in the polymer macromolecular chain.

DP1为聚合度为1的大分子,DP2为聚合度为2的大分子,DP3为聚合度为3的大分子。DP1 is a macromolecule with a degree of polymerization of 1, DP2 is a macromolecule with a degree of polymerization of 2, and DP3 is a macromolecule with a degree of polymerization of 3.

为了实现本发明,本发明采用如下技术方案:In order to realize the present invention, the present invention adopts following technical scheme:

一种抗性糊精,其特征在于:DP1的摩尔百分含量≤1%,DP2的摩尔百分含量≤4.5%,DP3的摩尔百分含量≤7.0%,平均聚合度为6~12,pH值3.0~6.0,膳食纤维摩尔百分含量≥85%。A resistant dextrin, characterized in that: the molar percentage of DP1 ≤ 1%, the molar percentage of DP2 ≤ 4.5%, the molar percentage of DP3 ≤ 7.0%, the average degree of polymerization is 6-12, the pH The value is 3.0-6.0, and the molar percentage of dietary fiber is ≥85%.

上述抗性糊精的制备方法,包括如下步骤:The preparation method of the above-mentioned resistant dextrin comprises the following steps:

(1)按质量百分比0.1%~0.5%的比例向淀粉中加入酸溶液,搅拌均匀,制得反应料;(1) adding an acid solution to the starch at a ratio of 0.1% to 0.5% by mass, and stirring evenly to obtain a reaction material;

(2)将步骤(1)制得的反应料升温至80℃~120℃,常压下反应2~4h,制得初反应料,然后按初反应料质量百分比1%~10%的比例加入酸溶液搅拌均匀,升温至140~200℃,常压条件下,糊化反应15~30min,制得糊精粗料;(2) Heat up the reaction material prepared in step (1) to 80°C to 120°C, react under normal pressure for 2 to 4 hours to obtain the initial reaction material, and then add Stir the acid solution evenly, raise the temperature to 140-200°C, and conduct a gelatinization reaction under normal pressure for 15-30 minutes to obtain coarse dextrin;

(3)向步骤(2)制得的糊精粗料中加入去离子水,调节糖浓度为40~45wt%,在温度为80~100℃条件下保温酸性水解1~2小时,制得水解液;(3) Add deionized water to the dextrin crude material prepared in step (2), adjust the sugar concentration to 40-45 wt%, and keep it under acidic hydrolysis at a temperature of 80-100°C for 1-2 hours to obtain the hydrolyzed liquid;

(4)将步骤(3)制得的水解液经脱色、离交、浓缩、纯化、干燥,制得抗性糊精。(4) The hydrolyzate obtained in step (3) is decolorized, separated, concentrated, purified, and dried to obtain resistant dextrin.

根据本发明优选的,所述步骤(1)和步骤(2)中的酸为食用酸;进一步优选的,所述的酸选自柠檬酸、苹果酸、盐酸、磷酸、硫酸中的一种或两种以上的组合。Preferably according to the present invention, the acid in the step (1) and step (2) is an edible acid; further preferably, the acid is selected from one of citric acid, malic acid, hydrochloric acid, phosphoric acid, sulfuric acid or A combination of two or more.

根据本发明优选的,所述步骤(1)和步骤(2)中的酸的质量浓度为0.08~0.12%。Preferably according to the present invention, the mass concentration of the acid in the step (1) and step (2) is 0.08-0.12%.

根据本发明优选的,所述步骤(4)中的脱色,步骤如下:Preferably according to the present invention, the decolorization in the described step (4), the steps are as follows:

按干基质量的0.5%~1.5%加入活性炭,保温搅拌25~35min后,过滤,制得透光率≥95%的料液。Add activated carbon at 0.5% to 1.5% of the dry basis mass, heat and stir for 25 to 35 minutes, and then filter to obtain a feed solution with a light transmittance ≥ 95%.

根据本发明优选的,所述步骤(4)中的离交,步骤如下:Preferably according to the present invention, the detachment in the described step (4), the steps are as follows:

调节进柱前料液温度为35~55℃,出柱料液pH4.0~5.0,制得电导<100μs/cm、透光率≥98%的离交液;Adjust the temperature of the feed liquid before entering the column to 35-55°C, and the pH of the feed liquid out of the column to 4.0-5.0 to obtain a ionizing liquid with a conductance of <100 μs/cm and a light transmittance of ≥98%;

根据本发明优选的,所述步骤(4)中的浓缩为采用六效浓缩,浓缩至固形物质量百分比含量为50~60%。Preferably according to the present invention, the concentration in the step (4) adopts six-effect concentration, and concentrates to a solid content of 50-60% by mass.

根据本发明优选的,所述步骤(4)中的纯化包括色谱提纯、二次脱色、二次离交、二次浓缩。Preferably according to the present invention, the purification in the step (4) includes chromatographic purification, secondary decolorization, secondary separation, and secondary concentration.

根据本发明进一步优选的,所述色谱提纯为调pH6.0~7.0,然后经色谱分离系统进行色谱提纯,色谱分离运行条件为运行压力0.2~0.35MPa,温度50~70℃,水耗比1:(1.2~1.5),每小时进料1.2~1.5m3Further preferably according to the present invention, the chromatographic purification is to adjust the pH to 6.0-7.0, and then carry out chromatographic purification through the chromatographic separation system. The operating conditions of the chromatographic separation are operating pressure 0.2-0.35MPa, temperature 50-70°C, water consumption ratio 1 : (1.2~1.5), feeding 1.2~1.5m 3 per hour.

根据本发明进一步优选的,所述二次脱色为按干基质量的0.5%~1.5%加入活性炭,保温搅拌25~35min后,过滤;According to a further preferred embodiment of the present invention, the secondary decolorization is to add activated carbon at 0.5% to 1.5% of the dry basis mass, heat and stir for 25 to 35 minutes, and then filter;

根据本发明进一步优选的,所述二次离交,步骤如下:According to a further preferred method of the present invention, the steps of said secondary separation are as follows:

调节进柱前料液温度为35~55℃,出柱料液pH4.0~5.0,制得电导<100μs/cm、透光率≥98%的二次离交液;Adjust the temperature of the feed liquid before entering the column to 35-55°C, and the pH of the feed liquid out of the column to be 4.0-5.0 to obtain a secondary ion exchange liquid with a conductance of <100 μs/cm and a light transmittance of ≥98%;

根据本发明进一步优选的,所述二次浓缩:采用六效浓缩,浓缩至固形物质量百分比含量为50~60%,pH4.0~5.0,制得电导<100μs/cm、透光率≥98%;According to a further preferred aspect of the present invention, the secondary concentration: use six-effect concentration to concentrate to a solid content of 50-60% by mass, pH 4.0-5.0, and obtain a conductivity < 100 μs/cm, light transmittance ≥ 98 %;

根据本发明优选的,所述步骤(4)中的干燥为经带式真空干燥至水分质量百分比含量≤6%。Preferably according to the present invention, the drying in the step (4) is belt-type vacuum drying until the moisture mass percentage is ≤6%.

上述原料均为本领域普通市售产品,工艺步骤如无特殊说明,均可按本领域常规操作。The above-mentioned raw materials are common commercially available products in the field, and the process steps can be operated according to the routine in the field unless otherwise specified.

有益效果Beneficial effect

1、本发明以淀粉为原料,首次将糊精化反应分为两个阶段,有力地保证了聚合反应的聚合度,同时减少副反应的产生,大大减少纯化后续处理的难度;1. The present invention uses starch as a raw material, divides the dextrinization reaction into two stages for the first time, effectively guarantees the degree of polymerization of the polymerization reaction, reduces side reactions at the same time, and greatly reduces the difficulty of subsequent purification treatment;

2.本发明采用无酶催化反应,即在反应整个过程中不需要添加生物酶,在水解过程中利用本身存在的酸性环境自然水解,采用无酶催化反应一方面简化了反应流程,另一方面大大降低了生产成本及减少后续纯化处理的难度;2. The present invention adopts non-enzyme catalyzed reaction, namely does not need to add biological enzyme in the whole process of reaction, utilizes the acidic environment that itself exists to hydrolyze naturally in the hydrolysis process, adopts non-enzyme catalyzed reaction to simplify the reaction process on the one hand, on the other hand Greatly reduce the production cost and reduce the difficulty of subsequent purification treatment;

3.本发明克服了原有工艺副反应多,产品苦味大、易潮解、流动性差等缺点,所制得的抗性糊精DP1的摩尔百分含量≤1%,DP2的摩尔百分含量≤4.5%,DP3的摩尔百分含量≤7.0%,平均聚合度为6~12,pH值3.0~6.0,膳食纤维摩尔百分含量≥85%,使得产品具有良好的口感和流动性,便于在食品、保健品尤其是高端食品和保健品领域广泛应用。3. The present invention overcomes the disadvantages of many side reactions in the original process, high bitterness of the product, easy deliquescence, and poor fluidity. The molar percentage of the prepared resistant dextrin DP1 is ≤ 1%, and the molar percentage of DP2 is ≤ 4.5%, the molar percentage of DP3 is ≤7.0%, the average degree of polymerization is 6-12, the pH value is 3.0-6.0, and the molar percentage of dietary fiber is ≥85%, which makes the product have good taste and fluidity, and is easy to use in food , health products, especially high-end food and health products are widely used.

具体实施方式detailed description

下面结合实施例对本发明的技术方案做进一步说明,但本发明所保护范围不限于此。The technical solutions of the present invention will be further described below in conjunction with the examples, but the protection scope of the present invention is not limited thereto.

实施例中所述的淀粉购自山东福洋生物科技.有限公司;The starch described in the examples was purchased from Shandong Fuyang Biotechnology Co., Ltd.;

苹果酸购自南京国海生物工程有限公司;Malic acid was purchased from Nanjing Guohai Biological Engineering Co., Ltd.;

柠檬酸购自山东柠檬生化有限公司。Citric acid was purchased from Shandong Lemon Biochemical Co., Ltd.

实施例1Example 1

抗性糊精的制备方法,包括如下步骤:The preparation method of resistant dextrin comprises the steps of:

(1)按质量百分比0.2%的比例向淀粉中加入苹果酸溶液,搅拌均匀,制得反应料;(1) Add malic acid solution to the starch at a ratio of 0.2% by mass, and stir evenly to obtain a reaction material;

(2)将步骤(1)制得的反应料升温至85℃,常压下反应2.5h,制得初反应料,然后按初反应料质量百分比2%的比例加入苹果酸溶液,搅拌均匀,升温至160℃,常压条件下,糊化反应20min,制得糊精粗料;(2) The reaction material obtained in step (1) is warmed up to 85° C., and reacted under normal pressure for 2.5 hours to obtain the initial reaction material, then add malic acid solution in a ratio of 2% by mass percent of the initial reaction material, and stir evenly. Raise the temperature to 160°C, under normal pressure, gelatinize for 20 minutes to obtain crude dextrin;

(3)向步骤(2)制得的糊精粗料中加入去离子水,调节糖浓度为41wt%,在温度为85℃条件下保温酸性水解1.2小时,制得水解液;(3) Add deionized water to the crude dextrin material prepared in step (2), adjust the sugar concentration to 41 wt%, and heat-preserve and acidify it for 1.2 hours at a temperature of 85°C to obtain a hydrolyzate;

(4)将步骤(3)制得的水解液经按干基质量的0.7%加入活性炭,保温搅拌30min后,过滤,制得透光率96%的料液;(4) The hydrolyzed solution prepared in step (3) is added activated carbon by 0.7% of the dry basis mass, and after insulated and stirred for 30min, it is filtered to obtain a feed solution with a light transmittance of 96%;

然后调节进柱前料液温度为41℃,出柱料液pH4.2,制得电导80μs/cm、透光率99%的离交液;Then adjust the temperature of the feed liquid before entering the column to be 41° C., and the pH of the feed liquid out of the column is 4.2, so as to obtain an ionizing liquid with a conductance of 80 μs/cm and a light transmittance of 99%.

然后采用六效浓缩,浓缩至固形物质量百分比含量为52%;Then adopt six-effect concentration, concentrate to solid matter percentage content and be 52%;

再经过色谱提纯、二次脱色、二次离交、二次浓缩,经带式真空干燥至水分质量百分比含量为5%,制得抗性糊精。After chromatographic purification, secondary decolorization, secondary separation, secondary concentration, and belt vacuum drying until the moisture content is 5%, the resistant dextrin is obtained.

所述色谱提纯为调pH6.5,然后经色谱分离系统进行色谱提纯,色谱分离运行条件为运行压力0.2MPa,温度50~70℃,水耗比1:1.2,每小时进料1.2m3The chromatographic purification is to adjust the pH to 6.5, and then perform chromatographic purification through the chromatographic separation system. The operating conditions of the chromatographic separation are operating pressure 0.2MPa, temperature 50-70°C, water consumption ratio 1:1.2, and feed 1.2m 3 per hour;

所述二次脱色为按干基质量的0.6%加入活性炭,保温搅拌30min后,过滤;The secondary decolorization is to add activated carbon according to 0.6% of the dry basis mass, and then filter after insulated and stirred for 30 minutes;

所述二次离交,步骤如下:Described secondary separation, the steps are as follows:

调节进柱前料液温度为39℃,出柱料液pH4.2,制得电导90μs/cm、透光率99%的二次离交液;Adjust the temperature of the feed liquid before entering the column to 39°C, and the pH of the feed liquid out of the column to 4.2, to obtain a secondary ion exchange liquid with a conductance of 90 μs/cm and a light transmittance of 99%.

所述二次浓缩:采用六效浓缩,浓缩至固形物质量百分比含量为55%,pH:4.5,电导<80μs/cm,透光率≥99%;The secondary concentration: using six-effect concentration, concentrated to a solid content of 55% by weight, pH: 4.5, conductance<80μs/cm, light transmittance≥99%;

所述步骤(1)和步骤(2)中的酸的质量浓度为0.1%。The mass concentration of the acid in the step (1) and the step (2) is 0.1%.

经检测,制得的抗性糊精DP1的摩尔百分含量为0.3%,DP2的摩尔百分含量为4.1%,DP3的摩尔百分含量为6%,平均聚合度为7,pH5.0,膳食纤维质量百分含量88%。After testing, the molar percentage of the prepared resistant dextrin DP1 is 0.3%, the molar percentage of DP2 is 4.1%, the molar percentage of DP3 is 6%, the average degree of polymerization is 7, pH5.0, The mass percentage content of dietary fiber is 88%.

实施例2Example 2

抗性糊精的制备方法,包括如下步骤:The preparation method of resistant dextrin comprises the steps of:

(1)按质量百分比0.1%的比例向淀粉中加入柠檬酸溶液,搅拌均匀,制得反应料;(1) Add citric acid solution to the starch at a ratio of 0.1% by mass, stir evenly, and prepare the reaction material;

(2)将步骤(1)制得的反应料升温至80℃,常压下反应2h,制得初反应料,然后按初反应料质量百分比2%的比例加入柠檬酸溶液搅拌均匀,升温至150℃,常压条件下,糊化反应17min,制得糊精粗料;(2) The reaction material that step (1) is made is warmed up to 80 ℃, reacts 2h under normal pressure, makes primary reaction material, then adds citric acid solution and stirs evenly by the ratio of initial reaction material mass percentage 2%, is heated up to 150°C, under normal pressure conditions, gelatinization reaction for 17min, to obtain crude dextrin;

(3)向步骤(2)制得的糊精粗料中加入去离子水,调节糖浓度为42wt%,在温度为85℃条件下保温酸性水解1.5小时,制得水解液;(3) Add deionized water to the crude dextrin material prepared in step (2), adjust the sugar concentration to 42 wt%, and heat-preserve the acidic hydrolysis at a temperature of 85° C. for 1.5 hours to obtain a hydrolyzed solution;

(4)将步骤(3)制得的水解液经按干基质量的0.7%加入活性炭,保温搅拌30min后,过滤,制得透光率96%的料液;(4) The hydrolyzed solution prepared in step (3) is added activated carbon by 0.7% of the dry basis mass, and after insulated and stirred for 30min, it is filtered to obtain a feed solution with a light transmittance of 96%;

然后调节进柱前料液温度为40℃,出柱料液pH4.5,制得电导90μs/cm、透光率98%的离交液;Then adjust the temperature of the feed liquid before entering the column to be 40°C, and the pH of the feed liquid out of the column is 4.5, so as to obtain a ion exchange liquid with a conductance of 90 μs/cm and a light transmittance of 98%.

然后采用六效浓缩,浓缩至固形物质量百分比含量为55%;Then adopt six-effect concentration to concentrate to a solid content of 55% by weight;

再经过色谱提纯、二次脱色、二次离交、二次浓缩,经带式真空干燥至水分质量百分比含量5%,制得抗性糊精。After chromatographic purification, secondary decolorization, secondary separation, secondary concentration, and belt vacuum drying to a moisture content of 5%, the resistant dextrin is obtained.

所述色谱提纯为调pH6.5,然后经色谱分离系统进行色谱提纯,色谱分离运行条件为运行压力0.35MPa,温度70℃,水耗比1:1.5,每小时进料1.5m3The chromatographic purification is to adjust the pH to 6.5, and then perform chromatographic purification through the chromatographic separation system. The operating conditions of the chromatographic separation are operating pressure 0.35MPa, temperature 70°C, water consumption ratio 1:1.5, and feed 1.5m 3 per hour;

所述二次脱色为按干基质量的0.7%加入活性炭,保温搅拌30min后,过滤;The secondary decolorization is to add activated carbon according to 0.7% of the dry mass, and then filter after insulated and stirred for 30 minutes;

所述二次离交,步骤如下:Described secondary separation, the steps are as follows:

调节进柱前料液温度为40℃,出柱料液pH4.5,制得电导80μs/cm、透光率99%的二次离交液;Adjust the temperature of the feed liquid before entering the column to 40°C, and the pH of the feed liquid out of the column to 4.5 to obtain a secondary ion exchange liquid with a conductance of 80 μs/cm and a light transmittance of 99%.

所述二次浓缩:采用六效浓缩,浓缩至固形物质量百分比含量为58%,pH4.5,电导90μs/cm,透光率99%;The secondary concentration: using six-effect concentration, concentrated to a solid content of 58% by mass, pH 4.5, conductance 90 μs/cm, and light transmittance 99%;

根据本发明优选的,所述步骤(1)和步骤(2)中的酸的质量浓度为0.08%。Preferably according to the present invention, the mass concentration of the acid in the step (1) and step (2) is 0.08%.

经检测,制得的抗性糊精DP1的摩尔百分含量为0.2%,DP2的摩尔百分含量为4.3%,DP3的摩尔百分含量为6.5%,平均聚合度为7,pH值4.0,膳食纤维质量百分含量90%。After testing, the molar percentage of the prepared resistant dextrin DP1 is 0.2%, the molar percentage of DP2 is 4.3%, the molar percentage of DP3 is 6.5%, the average degree of polymerization is 7, and the pH value is 4.0. Dietary fiber mass percentage content 90%.

实施例3Example 3

抗性糊精的制备方法,包括如下步骤:The preparation method of resistant dextrin comprises the steps of:

(1)按质量百分比0.3%的比例向淀粉中加入盐酸溶液,搅拌均匀,制得反应料;(1) adding hydrochloric acid solution to the starch at a ratio of 0.3% by mass, stirring evenly to obtain a reaction material;

(2)将步骤(1)制得的反应料升温至100℃,常压下反应3h,制得初反应料,然后按初反应料质量百分比6%的比例加入盐酸溶液搅拌均匀,升温至160℃,常压条件下,糊化反应22min,制得糊精粗料;(2) The reaction material prepared in step (1) is warmed up to 100° C., and reacted for 3 hours under normal pressure to obtain the initial reaction material, then add hydrochloric acid solution in a ratio of 6% by mass percent of the initial reaction material and stir evenly, and heat up to 160 ℃, under normal pressure conditions, gelatinization reaction for 22min, to obtain crude dextrin;

(3)向步骤(2)制得的糊精粗料中加入去离子水,调节糖浓度为43wt%,在温度为91℃条件下保温酸性水解1.5小时,制得水解液;(3) Add deionized water to the dextrin coarse material prepared in step (2), adjust the sugar concentration to 43wt%, and heat-preserve the acidic hydrolysis at a temperature of 91° C. for 1.5 hours to obtain a hydrolyzate;

(4)将步骤(3)制得的水解液经按干基质量的1.0%加入活性炭,保温搅拌30min后,过滤,制得透光率96%的料液;(4) The hydrolyzate prepared in step (3) was added activated carbon by 1.0% of the dry basis mass, and after insulated and stirred for 30 minutes, filtered to obtain a feed liquid with a light transmittance of 96%;

然后调节进柱前料液温度为45℃,出柱料液pH4.5,制得电导<100μs/cm、透光率≥98%的离交液;Then adjust the temperature of the feed liquid before entering the column to be 45°C, and the pH of the feed liquid out of the column to be 4.5, so as to obtain an ionizing liquid with a conductance of <100 μs/cm and a light transmittance of ≥98%;

然后采用六效浓缩,浓缩至固形物质量百分比含量为55%;Then adopt six-effect concentration to concentrate to a solid content of 55% by weight;

再经过色谱提纯、二次脱色、二次离交、二次浓缩,经带式真空干燥至水分质量百分比含量5%,制得抗性糊精。After chromatographic purification, secondary decolorization, secondary separation, secondary concentration, and belt vacuum drying to a moisture content of 5%, the resistant dextrin is obtained.

所述色谱提纯为调pH6.5,然后经色谱分离系统进行色谱提纯,色谱分离运行条件为运行压力0.3MPa,温度60℃,水耗比1:1.3,每小时进料1.4m3The chromatographic purification is to adjust the pH to 6.5, and then perform chromatographic purification through the chromatographic separation system. The operating conditions of the chromatographic separation are operating pressure 0.3MPa, temperature 60°C, water consumption ratio 1:1.3, and feed 1.4m 3 per hour;

所述二次脱色为按干基质量的1%加入活性炭,保温搅拌30min后,过滤;The secondary decolorization is to add activated carbon according to 1% of the dry mass, and after stirring for 30 minutes, filter;

所述二次离交,步骤如下:Described secondary separation, the steps are as follows:

调节进柱前料液温度为50℃,出柱料液pH4.5,制得电导85μs/cm、透光率99%的二次离交液;Adjust the temperature of the feed liquid before entering the column to 50°C, and the pH of the feed liquid out of the column to 4.5 to obtain a secondary ion exchange liquid with a conductivity of 85 μs/cm and a light transmittance of 99%.

所述二次浓缩:采用六效浓缩,浓缩至固形物质量百分比含量为60%,pH4.5,电导90μs/cm,透光率99%;The secondary concentration: using six-effect concentration, concentrated to a solid content of 60% by mass, pH 4.5, conductance 90 μs/cm, and light transmittance 99%;

所述步骤(1)和步骤(2)中的酸的质量浓度为0.12%。The mass concentration of the acid in the step (1) and step (2) is 0.12%.

经检测,制得的抗性糊精DP1的摩尔百分含量为0.5%,DP2的摩尔百分含量为4.1%,DP3的摩尔百分含量为6.0%,平均聚合度为9,pH 3.5,膳食纤维质量百分含量86%。After testing, the molar percentage of the prepared resistant dextrin DP1 is 0.5%, the molar percentage of DP2 is 4.1%, the molar percentage of DP3 is 6.0%, the average degree of polymerization is 9, pH 3.5, diet The fiber mass percentage is 86%.

实施例4Example 4

抗性糊精的制备方法,包括如下步骤:The preparation method of resistant dextrin comprises the steps of:

(1)按质量百分比0.5%的比例向淀粉中加入柠檬酸与苹果酸按体积比1:1的混合溶液,搅拌均匀,制得反应料;(1) Add a mixed solution of citric acid and malic acid in a volume ratio of 1:1 to the starch at a ratio of 0.5% by mass, and stir evenly to obtain a reaction material;

(2)将步骤(1)制得的反应料升温至120℃,常压下反应2h,制得初反应料,然后按初反应料质量百分比10%的比例加入柠檬酸与苹果酸按体积比1:1的混合溶液搅拌均匀,升温至200℃,常压条件下,糊化反应30min,制得糊精粗料;(2) The reaction material obtained in step (1) is heated up to 120° C., and reacted for 2 hours under normal pressure to obtain the initial reaction material, and then add citric acid and malic acid according to the volume ratio of the initial reaction material mass percentage of 10%. Stir the 1:1 mixed solution evenly, heat up to 200°C, and conduct a gelatinization reaction for 30 minutes under normal pressure to obtain coarse dextrin;

(3)向步骤(2)制得的糊精粗料中加入去离子水,调节糖浓度为45wt%,在温度为100℃条件下保温酸性水解2小时,制得水解液;(3) adding deionized water to the crude dextrin material prepared in step (2), adjusting the sugar concentration to 45 wt%, and keeping the temperature at 100° C. for 2 hours for acidic hydrolysis to obtain a hydrolyzed solution;

(4)将步骤(3)制得的水解液经按干基质量的1.5%加入活性炭,保温搅拌35min后,过滤,制得透光率95%的料液;(4) The hydrolyzate prepared in step (3) is added into activated carbon by 1.5% of the dry basis mass, and after insulated and stirred for 35min, filter to obtain a feed liquid with a light transmittance of 95%;

然后调节进柱前料液温度为55℃,出柱料液pH5.0,制得电导95μs/cm、透光率98%的离交液;Then adjust the temperature of the feed liquid before entering the column to be 55°C, and the pH of the feed liquid out of the column to be 5.0, to obtain an ionizing liquid with a conductance of 95 μs/cm and a light transmittance of 98%.

然后采用六效浓缩,浓缩至固形物质量百分比含量为60%;Then adopt six-effect concentration to concentrate to a solid content of 60% by weight;

再经过色谱提纯、二次脱色、二次离交、二次浓缩,经带式真空干燥至水分质量百分比含量6%,制得抗性糊精。After chromatographic purification, secondary decolorization, secondary separation, secondary concentration, and belt vacuum drying to a moisture content of 6%, the resistant dextrin is obtained.

所述色谱提纯为调pH7.0,然后经色谱分离系统进行色谱提纯,色谱分离运行条件为运行压力0.25MPa,温度65℃,水耗比1:1.4,每小时进料1.3m3The chromatographic purification is to adjust the pH to 7.0, and then perform chromatographic purification through the chromatographic separation system. The operating conditions of the chromatographic separation are operating pressure 0.25MPa, temperature 65°C, water consumption ratio 1:1.4, and feed 1.3m 3 per hour;

所述二次脱色为按干基质量的1.5%加入活性炭,保温搅拌35min后,过滤;The secondary decolorization is to add activated carbon according to 1.5% of the dry mass, and then filter after insulated and stirred for 35 minutes;

所述二次离交,步骤如下:Described secondary separation, the steps are as follows:

调节进柱前料液温度为55℃,出柱料液pH5.0,制得电导95μs/cm、透光率99%的二次离交液;Adjust the temperature of the feed liquid before entering the column to 55°C, and the pH of the feed liquid out of the column to 5.0 to obtain a secondary ion exchange liquid with a conductivity of 95 μs/cm and a light transmittance of 99%.

所述二次浓缩:采用六效浓缩,浓缩至固形物质量百分比含量为56%,pH5.0,电导95μs/cm,透光率99%;The secondary concentration: using six-effect concentration, concentrated to a solid content of 56% by mass, pH 5.0, conductance 95 μs/cm, and light transmittance 99%;

所述步骤(1)和步骤(2)中的酸的质量浓度为0.09%。The mass concentration of the acid in the step (1) and step (2) is 0.09%.

经检测,制得的抗性糊精DP1的摩尔百分含量为0.5%,DP2的摩尔百分含量为4.1%,DP3的摩尔百分含量为6.0%,平均聚合度为11,pH5.0,膳食纤维质量百分含量91%。After testing, the molar percentage of the prepared resistant dextrin DP1 is 0.5%, the molar percentage of DP2 is 4.1%, the molar percentage of DP3 is 6.0%, the average degree of polymerization is 11, pH5.0, The mass percentage content of dietary fiber is 91%.

实施例5Example 5

抗性糊精的制备方法,包括如下步骤:The preparation method of resistant dextrin comprises the steps of:

(1)按质量百分比0.1%的比例向淀粉中加入磷酸溶液,搅拌均匀,制得反应料;(1) adding phosphoric acid solution to the starch at a ratio of 0.1% by mass, stirring evenly to obtain a reaction material;

(2)将步骤(1)制得的反应料升温至80℃,常压下反应2h,制得初反应料,然后按初反应料质量百分比1%的比例加入磷酸溶液升温至140℃,常压条件下,糊化反应15min,制得糊精粗料;(2) The reaction material that step (1) is made is warmed up to 80 ℃, reacts 2h under normal pressure, makes initial reaction material, then adds phosphoric acid solution and is warming up to 140 ℃ by the ratio of initial reaction material mass percentage 1%, usually Under pressure conditions, the gelatinization reaction was carried out for 15 minutes, and the dextrin crude material was obtained;

(3)向步骤(2)制得的糊精粗料中加入去离子水,调节糖浓度为40wt%,在温度为80℃条件下保温酸性水解1小时,制得水解液;(3) adding deionized water to the crude dextrin material prepared in step (2), adjusting the sugar concentration to 40 wt%, and keeping the temperature at 80° C. for 1 hour for acidic hydrolysis to obtain a hydrolyzed solution;

(4)将步骤(3)制得的水解液经按干基质量的0.5%加入活性炭,保温搅拌25min后,过滤,制得透光率96%的料液;(4) The hydrolyzate prepared in step (3) was added activated carbon by 0.5% of the dry basis mass, and after insulated and stirred for 25 minutes, filtered to obtain a feed liquid with a light transmittance of 96%;

然后调节进柱前料液温度为35℃,出柱料液pH4.0,制得电导80μs/cm、透光率99%的离交液;Then adjust the temperature of the feed liquid before entering the column to be 35° C., and the pH of the feed liquid out of the column is 4.0, so as to obtain an ionizing liquid with a conductance of 80 μs/cm and a light transmittance of 99%.

然后采用六效浓缩,浓缩至固形物质量百分比含量为50%;Then adopt six-effect concentration, and concentrate until the mass percent content of solid matter is 50%;

再经过色谱提纯、二次脱色、二次离交、二次浓缩,经带式真空干燥至水分质量百分比含量6%,制得抗性糊精。After chromatographic purification, secondary decolorization, secondary separation, secondary concentration, and belt vacuum drying to a moisture content of 6%, the resistant dextrin is obtained.

所述色谱提纯为调pH6.0,然后经色谱分离系统进行色谱提纯,色谱分离运行条件为运行压力0.25MPa,温度55℃,水耗比1:1.25,每小时进料1.25m3The chromatographic purification is to adjust the pH to 6.0, and then perform chromatographic purification through the chromatographic separation system. The operating conditions of the chromatographic separation are operating pressure 0.25MPa, temperature 55°C, water consumption ratio 1:1.25, and feed 1.25m 3 per hour;

所述二次脱色为按干基质量的0.5%加入活性炭,保温搅拌25min后,过滤;The secondary decolorization is to add activated carbon according to 0.5% of the dry mass, and after stirring for 25 minutes, filter;

所述二次离交,步骤如下:Described secondary separation, the steps are as follows:

调节进柱前料液温度为35℃,出柱料液pH4.0,制得电导80μs/cm、透光率99%的二次离交液;Adjust the temperature of the feed liquid before entering the column to 35°C, and the pH of the feed liquid out of the column to 4.0 to obtain a secondary ion exchange liquid with a conductivity of 80 μs/cm and a light transmittance of 99%.

所述二次浓缩:采用六效浓缩,浓缩至固形物质量百分比含量为53%,pH4.0,电导80μs/cm,透光率99%;;The secondary concentration: using six-effect concentration, concentrated to a solid content of 53% by weight, pH 4.0, conductance 80 μs/cm, and light transmittance 99%;

所述步骤(1)和步骤(2)中的酸的质量浓度为0.11%。The mass concentration of the acid in the step (1) and step (2) is 0.11%.

经检测,制得的抗性糊精DP1的摩尔百分含量为1%,DP2的摩尔百分含量为4.5%,DP3的摩尔百分含量为7.0%,平均聚合度为6,pH值3.5,膳食纤维含量89%。After testing, the molar percentage of the prepared resistant dextrin DP1 is 1%, the molar percentage of DP2 is 4.5%, the molar percentage of DP3 is 7.0%, the average degree of polymerization is 6, and the pH value is 3.5. The dietary fiber content is 89%.

对比例1Comparative example 1

传统制备抗性糊精的工艺如下:The traditional process of preparing resistant dextrin is as follows:

向淀粉中加入重量百分比0.05~0.5%的盐酸溶液,混合均匀,过滤,预干燥,用打粉机粉碎后过20~60目筛,将食用油与预干燥后的淀粉混合均匀,然后将混合物加入到反应容器中温度升至150~250℃进行酸热反应10~120分钟,反应结束获得难消化糊精粗品,难消化糊精粗品再经过精制处理得到难消化糊精产品;Add 0.05-0.5% hydrochloric acid solution by weight to the starch, mix evenly, filter, pre-dry, pulverize with a powder machine and pass through a 20-60 mesh sieve, mix the edible oil and the pre-dried starch evenly, and then add the mixture The temperature in the reaction vessel is raised to 150-250°C for acid-heat reaction for 10-120 minutes, and the crude indigestible dextrin is obtained after the reaction is completed, and the crude indigestible dextrin is refined to obtain the indigestible dextrin product;

所述盐酸的质量浓度为0.1%。The mass concentration of the hydrochloric acid is 0.1%.

所述预干燥的温度为80℃~110℃,预干燥直至水分含量少于5wt%。The pre-drying temperature is 80° C. to 110° C., and the pre-drying is performed until the moisture content is less than 5 wt%.

所述食用油是食用大豆油。The edible oil is edible soybean oil.

所述食用油的加入量为淀粉重量的10~200%。The added amount of the edible oil is 10-200% of the weight of the starch.

对比例2Comparative example 2

抗性糊精的制备方法,包括如下步骤:A method for preparing resistant dextrin, comprising the steps of:

(1)按质量百分比6.3%的比例向淀粉中加入盐酸溶液搅拌均匀,升温至160℃,常压条件下,糊化反应3小时22分钟,制得糊精粗料;搅拌均匀,制得反应料;(1) Add hydrochloric acid solution to starch in a proportion of 6.3% by mass and stir evenly, heat up to 160°C, and under normal pressure, gelatinize for 3 hours and 22 minutes to obtain coarse dextrin; stir evenly to obtain reaction material;

(3)向步骤(2)制得的糊精粗料中加入去离子水,调节糖浓度为43wt%,在温度为91℃条件下保温酸性水解1.5小时,制得水解液;(3) Add deionized water to the dextrin coarse material prepared in step (2), adjust the sugar concentration to 43wt%, and heat-preserve the acidic hydrolysis at a temperature of 91° C. for 1.5 hours to obtain a hydrolyzate;

(4)将步骤(3)制得的水解液经按干基质量的1.0%加入活性炭,保温搅拌30min后,过滤,制得透光率96%的料液;(4) The hydrolyzate prepared in step (3) was added activated carbon by 1.0% of the dry basis mass, and after insulated and stirred for 30 minutes, filtered to obtain a feed liquid with a light transmittance of 96%;

然后调节进柱前料液温度为45℃,出柱料液pH4.5,制得电导<100μs/cm、透光率≥98%的离交液;Then adjust the temperature of the feed liquid before entering the column to be 45°C, and the pH of the feed liquid out of the column to be 4.5, so as to obtain an ionizing liquid with a conductance of <100 μs/cm and a light transmittance of ≥98%;

然后采用六效浓缩,浓缩至固形物质量百分比含量为55%;Then adopt six-effect concentration to concentrate to a solid content of 55% by weight;

再经过色谱提纯、二次脱色、二次离交、二次浓缩,经带式真空干燥至水分质量百分比含量5%,制得抗性糊精。After chromatographic purification, secondary decolorization, secondary separation, secondary concentration, and belt vacuum drying to a moisture content of 5%, the resistant dextrin is obtained.

所述色谱提纯为调pH6.5,然后经色谱分离系统进行色谱提纯,色谱分离运行条件为运行压力0.25MPa,温度55℃,水耗比1:1.25,每小时进料1.25m3The chromatographic purification is to adjust the pH to 6.5, and then perform chromatographic purification through the chromatographic separation system. The operating conditions of the chromatographic separation are operating pressure 0.25MPa, temperature 55°C, water consumption ratio 1:1.25, and feed 1.25m 3 per hour;

所述二次脱色为按干基质量的1%加入活性炭,保温搅拌30min后,过滤;The secondary decolorization is to add activated carbon according to 1% of the dry mass, and after stirring for 30 minutes, filter;

所述二次离交,步骤如下:Described secondary separation, the steps are as follows:

调节进柱前料液温度为50℃,出柱料液pH4.5,制得电导85μs/cm、透光率99%的二次离交液;Adjust the temperature of the feed liquid before entering the column to 50°C, and the pH of the feed liquid out of the column to 4.5 to obtain a secondary ion exchange liquid with a conductivity of 85 μs/cm and a light transmittance of 99%.

所述二次浓缩:采用六效浓缩,浓缩至固形物质量百分比含量为55%,pH4.5,电导90μs/cm,透光率99%;The secondary concentration: using six-effect concentration, concentrated to a solid content of 55% by mass, pH 4.5, conductance 90 μs/cm, and light transmittance 99%;

所述步骤(1)和步骤(2)中的酸的质量浓度为0.1%。The mass concentration of the acid in the step (1) and the step (2) is 0.1%.

经检测,制得的抗性糊精DP1为2.5%,DP2为8.1%,DP3为12.0%,平均聚合度为15,pH 3.5,膳食纤维质量百分含量62%。After testing, the prepared resistant dextrin has a DP1 of 2.5%, a DP2 of 8.1%, a DP3 of 12.0%, an average degree of polymerization of 15, a pH of 3.5, and a dietary fiber mass percentage of 62%.

应用例Application example

对比例1和对比例2产品与实施例3所制得的产品经检测产品指标对比如下:Comparative example 1 and comparative example 2 products and the product made by embodiment 3 compare as follows through testing product index:

膳食纤维含量检测依国家标准《GB/T 5009.88-2008食品中膳食纤维的测定》进行检测。Dietary fiber content is tested according to the national standard "GB/T 5009.88-2008 Determination of Dietary Fiber in Food".

表1Table 1

DP1DP1 DP2DP2 DP3DP3 平均聚合度Average degree of polymerization 膳食纤维含量Dietary Fiber Content 对比例1Comparative example 1 3.2%3.2% 8.5%8.5% 15.0%15.0% 21twenty one 58%58% 对比例2Comparative example 2 2.5%2.5% 8.1%8.1% 12%12% 1515 6262 实施例3Example 3 0.5%0.5% 4.1%4.1% 6.0%6.0% 99 86%86%

由以上对比可以看出,实施例3抗性糊精产品较对比例DP1-DP3含量低很多,而且平均聚合度低说明反应更加充分,分离量分布更加均匀,同时膳食纤维含量更高,产品性能优势明显。From the above comparison, it can be seen that the content of the resistant dextrin product in Example 3 is much lower than that of the comparative examples DP1-DP3, and the low average degree of polymerization indicates that the reaction is more sufficient, the distribution of separation is more uniform, and the content of dietary fiber is higher at the same time. The advantages are obvious.

对比例1和对比例2产品与实施例3所制得的产品应用性对比如下:Comparative example 1 and the product applicability contrast that comparative example 2 product and embodiment 3 make are as follows:

将实施例3抗性糊精产品与对比例和对比例2产品进行对比,产品流动性采用休止角指标进行对比评价,休止角是指粉末或颗粒堆积成最陡堆的斜边与水平面之间的夹角,流动性常以休止角表示,休止角小流动性好,否则相反。The resistant dextrin product of Example 3 was compared with the products of Comparative Example and Comparative Example 2. The fluidity of the product was compared and evaluated using the index of angle of repose. The included angle, the fluidity is often expressed by the angle of repose, the smaller the angle of repose, the better the fluidity, otherwise the opposite.

吸潮性(吸湿率)按如下公式计算:Hygroscopicity (moisture absorption rate) is calculated according to the following formula:

吸湿率=(吸湿后样品质量-绝干样品质量)/绝干样品质量Moisture absorption rate = (sample mass after moisture absorption - absolute dry sample mass) / absolute dry sample mass

检测结果如下表2所示:The test results are shown in Table 2 below:

表2Table 2

由上述数据可以看出,对比例1和对比例2由于DP1、DP2和DP3均不符合DP1的摩尔百分含量≤1%,DP2的摩尔百分含量≤4.5%,DP3的摩尔百分含量≤7.0%的要求,且平均聚合度未满足6~12的要求,因此其在口味、流动性、溶解度、吸潮性等方面均显著不及实施例3的产品指标。As can be seen from the above data, Comparative Example 1 and Comparative Example 2 do not comply with the molar percentage of DP1 ≤ 1% due to DP1, DP2 and DP3, the molar percentage of DP2 ≤ 4.5%, and the molar percentage of DP3 ≤ 4.5%. 7.0% requirement, and the average polymerization degree does not meet the requirement of 6~12, so it is all significantly inferior to the product index of embodiment 3 in respects such as taste, fluidity, solubility, hygroscopicity.

Claims (12)

1. a kind of preparation method of resistant dextrin, it is characterised in that comprise the following steps:
(1)0.1%~0.5% ratio adds acid solution into starch by mass percentage, stirs, and reaction material is made;
(2)By step(1)Obtained reaction material is warming up to 80 DEG C~120 DEG C, and 2~4h is reacted under normal pressure, initial action material is made, so Acid solution is added in the ratio of initial action material mass percent 1%~10% to stir, be warming up to 140~200 DEG C, normal pressure bar afterwards Under part, dextrin coarse fodder is made in gelatinization 15~30min of reaction;
(3)To step(2)Deionized water is added in obtained dextrin coarse fodder, the sugared concentration of regulation is 40~45wt%, be 80 in temperature Acidic hydrolysis 1~2 hour is incubated under the conditions of~100 DEG C, hydrolyzate is made;
(4)By step(3)Obtained hydrolyzate is through decolouring, from friendship, concentration, purifying, dry, obtained resistant dextrin;
The Mole percent of molar content≤4.5%, DP3 of molar content≤1%, DP2 of the resistant dextrin DP1 contains Amount≤7.0%, average degree of polymerization is 6~12, pH value 3.0~6.0, dietary fiber molar content >=85%.
2. preparation method as claimed in claim 1, it is characterised in that the step(1)And step(2)In acid be selected from lemon Combination more than one or both of acid, malic acid, hydrochloric acid, phosphoric acid, sulfuric acid.
3. preparation method as claimed in claim 1, it is characterised in that the step(1)And step(2)In acid solution matter It is 0.08~0.12% to measure concentration.
4. preparation method as claimed in claim 1, it is characterised in that the step(4)In decolouring, step is as follows:
Added by the 0.5%~1.5% of butt quality after activated carbon, 25~35min of insulated and stirred, light transmittance >=95% is made in filtering Feed liquid.
5. preparation method as claimed in claim 1, it is characterised in that the step(4)In from friendship, step is as follows:
It is 35~55 DEG C to adjust the feed temperature into before post, goes out post material liquid pH 4.0~5.0, and the μ s/cm of conductance < 100, light transmittance is made >=98% from hand over liquid.
6. preparation method as claimed in claim 1, it is characterised in that the step(4)In concentration be using six effect concentrate, It is 50~60% to be concentrated into solid quality degree.
7. preparation method as claimed in claim 1, it is characterised in that the step(4)In purifying include chromatography purity, two It is secondary decolourize, it is secondary from hand over, secondary concentration.
8. preparation method as claimed in claim 7, it is characterised in that the chromatography purity is tune pH6.0~7.0, Ran Houjing Chromatographic fractionation system carry out chromatography purity, chromatographic isolation service condition be 0.2~0.35MPa of operating pressure, 50~70 DEG C of temperature, Water consume compares 1:(1.2~1.5), 1.2~1.5m is fed per hour3
9. preparation method as claimed in claim 7, it is characterised in that the secondary decolourization be by butt quality 0.5%~ 1.5% adds after activated carbon, 25~35min of insulated and stirred, filtering.
10. preparation method as claimed in claim 7, it is characterised in that described secondary from friendship, step is as follows:
It is 35~55 DEG C to adjust the feed temperature into before post, goes out post material liquid pH 4.0~5.0, and the μ s/cm of conductance < 100, light transmittance is made >=98% it is secondary from hand over liquid.
11. preparation method as claimed in claim 7, it is characterised in that the secondary concentration:Concentrated, be concentrated into using six effects Solid quality degree is 50~60%, pH4.0~5.0, and the μ s/cm of conductance < 100, light transmittance >=98% is made.
12. preparation method as claimed in claim 1, it is characterised in that the step(4)In drying be dry through belt vacuum It is dry to biodiversity degree≤6%.
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Families Citing this family (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102186886B (en) 2008-08-20 2015-08-19 卡吉尔公司 New polydextrose material
CN105542019B (en) * 2016-01-27 2017-08-18 山东百龙创园生物科技股份有限公司 Resistant dextrin and preparation method thereof
KR101832799B1 (en) * 2016-05-19 2018-02-27 주식회사 삼양사 Method for preparing digestion-resistant maltodextrin
CN106173962A (en) * 2016-06-27 2016-12-07 郑州国食科技有限公司 A kind of preparation method containing resistant dextrin huyashi-chuuka (cold chinese-style noodles)
CN106318991A (en) * 2016-08-19 2017-01-11 山东百龙创园生物科技有限公司 Resistant dextrin and preparation method thereof
CN106755203A (en) * 2016-11-28 2017-05-31 保龄宝生物股份有限公司 A kind of preparation method of resistant dextrin
CN107384989A (en) * 2017-07-20 2017-11-24 江南大学 A kind of branching enzyme and its application in resistant dextrin preparation
CN109438583B (en) * 2018-11-26 2021-07-13 黑龙江八一农垦大学 A method for purifying resistant dextrin by sequential simulated mobile chromatography
CN111455002A (en) * 2020-04-14 2020-07-28 曲阜贝斯迪生物医药有限公司 Preparation method of resistant dextrin
CN112480276B (en) * 2020-12-31 2021-11-26 保龄宝生物股份有限公司 Energy-saving and environment-friendly production process of high-light-transmittance resistant dextrin
EP4272577A4 (en) * 2020-12-31 2024-11-13 Samyang Corporation DEXTRIN WITH IMPROVED TURBIDITY AND PROCESS FOR PRODUCTION THEREOF
CN114262387B (en) * 2021-12-29 2022-09-30 山东百龙创园生物科技股份有限公司 Preparation method of resistant dextrin
CN118679190A (en) 2022-02-17 2024-09-20 嘉吉公司 Resistant dextrins and methods of making resistant dextrins
WO2023159172A1 (en) 2022-02-17 2023-08-24 Cargill, Incorporated Resistant dextrins and methods of making resistant dextrins
CN118696065A (en) 2022-02-17 2024-09-24 嘉吉公司 Resistant dextrin and method for preparing resistant dextrin
US20250136723A1 (en) 2022-02-17 2025-05-01 Cargill, Incorporated Resistant dextrins and methods of making resistant dextrins
WO2024036206A1 (en) 2022-08-12 2024-02-15 Cargill, Incorporated Polycondensation of sugars in the presence of water using a microreactor
CN119286955B (en) * 2024-12-11 2025-03-04 山东百龙创园生物科技股份有限公司 High dietary fiber content resistant dextrin and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013015890A1 (en) * 2011-07-26 2013-01-31 Grain Processing Corporation Production of resistant dextrins
CN103725732A (en) * 2013-12-28 2014-04-16 郑州市中食农产品加工研究院 Method for preparing resistant dextrin employing comprehensive utilization of wheat C starch
CN104403009A (en) * 2014-11-21 2015-03-11 广东省食品工业研究所 Preparation method of resistant dextrin
CN104561191A (en) * 2014-12-30 2015-04-29 山东百龙创园生物科技有限公司 Preparation method of resistant dextrin
CN105237647A (en) * 2015-11-20 2016-01-13 保龄宝生物股份有限公司 Method for preparing high-purity resistant dextrin by improving acidity

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU433489B2 (en) * 1968-08-14 1973-03-08 Starch hydrolysis
JPH04173094A (en) 1990-11-08 1992-06-19 Matsutani Kagaku Kogyo Kk Production of low calorie dextrin
JPH05178902A (en) 1991-10-29 1993-07-20 Matsutani Kagaku Kogyo Kk Difficultly digestible dextrin
JPH09278802A (en) 1996-04-16 1997-10-28 Nakano Vinegar Co Ltd Method for producing aging resistant starch
JP2005263867A (en) 2004-03-16 2005-09-29 Oji Cornstarch Co Ltd Roast dextrin with high content of dietary fiber and its preparation method
JP5491415B2 (en) 2008-02-01 2014-05-14 ユニリーバー・ナームローゼ・ベンノートシヤープ Water-soluble carrier
FR2987360B1 (en) 2012-02-28 2014-03-28 Roquette Freres HYPER-GLYCEMIANT HYPERBRANCHE MALTODEXTRINS
CN102960741B (en) * 2012-11-02 2014-05-14 翁源广业清怡食品科技有限公司 Preparation process of indigestible dextrin
CA2906984A1 (en) 2013-03-15 2014-09-18 Cargill, Incorporated Carbohydrate compositions
CN105542019B (en) * 2016-01-27 2017-08-18 山东百龙创园生物科技股份有限公司 Resistant dextrin and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013015890A1 (en) * 2011-07-26 2013-01-31 Grain Processing Corporation Production of resistant dextrins
CN103725732A (en) * 2013-12-28 2014-04-16 郑州市中食农产品加工研究院 Method for preparing resistant dextrin employing comprehensive utilization of wheat C starch
CN104403009A (en) * 2014-11-21 2015-03-11 广东省食品工业研究所 Preparation method of resistant dextrin
CN104561191A (en) * 2014-12-30 2015-04-29 山东百龙创园生物科技有限公司 Preparation method of resistant dextrin
CN105237647A (en) * 2015-11-20 2016-01-13 保龄宝生物股份有限公司 Method for preparing high-purity resistant dextrin by improving acidity

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
尹月玲,张 姝,王明珠等.抗牲糊精的研究进展及市场现状.《精细与专用化学品》.2012,第20卷(第l2期),第35页. *

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